ChemicalBook CAS DataBase List diisobutyl hydrogen phosphate

diisobutyl hydrogen phosphate synthesis

7synthesis methods

Product Name:diisobutyl hydrogen phosphate
CAS Number:6303-30-6
Molecular formula:C8H19O4P
Molecular Weight:210.21

1-(chloro-(2-Methylpropoxy)phosphoryl)oxy-2-Methyl-propane

17158-87-1
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6303-30-6
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Yield:6303-30-6 75%

Reaction Conditions:

with sodium hydroxide in tetrahydrofuran;water at 0;

Steps:

General procedure 2: synthesis of dialkyl hydrogen phosphates

General procedure: The corresponding alky chlorophosphate (1 equiv.) was dissolved in THF and the resulting colorless solution was cooled to 0 °C. Then, aqueous NaOH (1 M, 1 equiv.) was added dropwise. The resulting mixture was stirred vigorously at 0 °C for 30 min, then concentrated under reduced pressure. The residual wet white solid was extracted with Et₂O and the organic layer was dried over MgSO₄. After filtration, the resulting solution was concentrated under reduced pressure to yield the crude product as a viscous oil. The latter was dissolved in a saturated solution of NaHCO₃ that was subsequently washed three times with the same amount of CH₂Cl₂. The aqueous layer was then acidified with HCl (1 M) until the pH value was between 0 and 1 and extracted with CH₂Cl₂ (3× 50 mL). The combined organic layers were dried over MgSO₄, then concentrated under reduced pressure to yield pure dialkyl hydrogen phosphates. All products were stored at -17 °C under an atmosphere of argon. All characterization data can be found in the electronic supplementary information.

References:

Santschi, Nico;Geissbühler, Patrik;Togni, Antonio [Journal of Fluorine Chemistry,2012,vol. 135,p. 83 - 86] Location in patent:experimental part

126-71-6 Synthesis